WO2023152353A1 - Procédé et appareil d'adaptation de réglages d'opération d'une mesure de balayage de fréquence d'un produit polymère - Google Patents

Procédé et appareil d'adaptation de réglages d'opération d'une mesure de balayage de fréquence d'un produit polymère Download PDF

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Publication number
WO2023152353A1
WO2023152353A1 PCT/EP2023/053435 EP2023053435W WO2023152353A1 WO 2023152353 A1 WO2023152353 A1 WO 2023152353A1 EP 2023053435 W EP2023053435 W EP 2023053435W WO 2023152353 A1 WO2023152353 A1 WO 2023152353A1
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WO
WIPO (PCT)
Prior art keywords
frequency range
measurement
optimized
frequency
polymer product
Prior art date
Application number
PCT/EP2023/053435
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English (en)
Inventor
Vasileios TOULOUPIDIS
Bernhard Knogler
Vitor Barroso
Anna-Karin Jarl
Christoph Kaufmann
Niclas Carlsson
Staffan Skalen
Original Assignee
Borealis Ag
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by Borealis Ag filed Critical Borealis Ag
Publication of WO2023152353A1 publication Critical patent/WO2023152353A1/fr

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/44—Resins; rubber; leather
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties

Definitions

  • the present invention relates to methods for polymer rheological characterization via fast frequency sweep and in particular to a method and an apparatus for adapting operation settings for a frequency sweep measurement of a polymer product.
  • reactor sample In order to monitor and control the properties of a polymer during production, reactor sample needs to be collected and characterized with a material- or parametercharacterizing method of choice at regular intervals, defining the manipulative moves.
  • the measurement feedback frequency for classic common-use reactors typically every 4 to 6 hours, limits the selection of the characterization methods only to those that can provide results within this timeframe. For instance, the total measurement time includes sample acquisition, sample preparation, measurement preparation, sample heating-up, and actual measurement. Furthermore, additional limitations connected to technical expertise level and plant resources further apply.
  • a method for adapting operation settings for a frequency sweep measurement of a polymer product.
  • the method comprises the step of providing at least one set of operation setting parameters comprising at least one frequency range for the frequency sweep measurement of the polymer product, the at least one frequency range comprising a plurality of specific measurement frequencies.
  • the method comprises the step of optimizing the frequency range by deleting at least one measurement frequency of the plurality of specific measurement frequencies within a lower half of the frequency range resulting in a first optimized frequency range.
  • the method comprises the step of optimizing the first optimized frequency range by determining a value of measurement frequencies present per decade of frequency within at least a subrange of the frequency range and reducing the determined value of measurement frequencies present per decade within the at least one subrange of the frequency range by deleting at least one measurement frequency of the at least one subrange resulting in a second optimized frequency range.
  • the present invention advantageously provides a set of special operation settings for the frequency sweep measurement that leads to significant reduction of measurement time while the method accuracy remains at an adequate level for the needs of plant control.
  • the present invention advantageously allows that the settings lead to significant reduction of the measurement time.
  • the first optimized frequency range is further optimized by equally distributing the remaining specific measurement frequencies within the lower half of the frequency range or within the complete frequency range.
  • the second optimized frequency range is further optimized by equally distributing the remaining specific measurement frequencies within the subrange of the frequency range or within the complete frequency range.
  • the method further comprises the step of validating a consistency of the second optimized frequency range by comparing a calculated complex viscosity value to a measured melt flow index value using the second optimized frequency range.
  • the method further comprises the steps of applying the second optimized frequency range for quality control measurements of the polymer product.
  • the method further comprises the steps of applying the second optimized frequency range for a currently employed melt flow index measurement. This step might be combined with the previously mentioned step of applying the second optimized frequency range for quality control measurements of the polymer product.
  • the method further comprises the steps of generating the second optimized frequency range for a specific polymer grade of interest of the polymer product.
  • a frequency sweep fingerprint for the specific polymer grade is defined.
  • the set of operation setting parameters comprises at least one shear rate.
  • a computer program product comprising computer-readable instructions which, when loaded and executed on processor, performs the method according to any one of the embodiments of the first aspect or the first aspect as such.
  • an apparatus configured for adapting operation settings for a frequency sweep measurement of a polymer product, the apparatus comprising a data memory and a processor.
  • the data memory is configured to provide at least one set of operation setting parameters comprising at least one frequency range for the frequency sweep measurement of the polymer product, the at least one frequency range comprising a plurality of specific measurement frequencies.
  • the processor is configured to optimize the frequency range by deleting at least one measurement frequency of the plurality of specific measurement frequencies within a lower half of the frequency range resulting in a first optimized frequency range.
  • the processor is configured to optimize the first optimized frequency range by determining a value of measurement frequencies present per decade of frequency within at least a subrange of the frequency range and reducing the determined value of measurement frequencies present per decade within the at least one subrange of the frequency range by deleting at least one measurement frequency of the at least one subrange resulting in a second optimized frequency range.
  • the processor is further configured to optimize the first optimized frequency range by equally distributing the remaining specific measurement frequencies within the lower half of the frequency range or within the complete frequency range.
  • the processor is further configured to optimize the second optimized frequency range by equally distributing the remaining specific measurement frequencies within the subrange of the frequency range or within the complete frequency range.
  • the processor is further configured apply the second optimized frequency range for quality control measurements of the polymer product.
  • the processor is further configured to apply the second optimized frequency range for a currently employed melt flow index measurement.
  • a computer program performing the method of the present invention may be stored on a computer-readable medium.
  • a computer-readable medium may be a floppy disk, a hard disk, a CD, a DVD, an USB (Universal Serial Bus) storage device, a RAM (Random Access Memory), a ROM (Read Only Memory) and an EPROM (Erasable Programmable Read Only Memory).
  • a computer-readable medium may also be a data communication network, for example the Internet, which allows downloading a program code, with a connection via WLAN or 3G/4G or any other wireless data technology.
  • the methods, systems and devices described herein may be implemented as software in a Digital Signal Processor, DSP, in a micro-controller or in any other sideprocessor or as hardware circuit within an application specific integrated circuit, ASIC, CPLD or FPGA.
  • DSP Digital Signal Processor
  • ASIC application specific integrated circuit
  • CPLD CPLD
  • FPGA field-programmable gate array
  • Fig. 1 shows a schematic diagram of a method for adapting operation settings for a frequency sweep measurement of a polymer product according to an exemplary embodiment of the invention
  • Fig. 2 shows a schematic diagram of an apparatus for adapting operation settings for a frequency sweep measurement of a polymer product according to an exemplary embodiment of the invention.
  • Fig. 1 shows a schematic diagram of a method for adapting operation settings for a frequency sweep measurement of a polymer product according to an exemplary embodiment of the invention.
  • Fig. 1 shows a method for adapting operation settings for a frequency sweep measurement of a polymer product, the method comprising the following steps.
  • providing SI at least one set of operation setting parameters comprising at least one frequency range for the frequency sweep measurement of the polymer product, the at least one frequency range comprising a plurality of specific measurement frequencies is conducted.
  • optimizing S2 the frequency range by deleting at least one measurement frequency of the plurality of specific measurement frequencies within a lower half of the frequency range resulting in a first optimized frequency range is performed.
  • optimizing S3 the first optimized frequency range by determining a value of measurement frequencies present per decade of frequency within at least a subrange of the frequency range and reducing the determined value of measurement frequencies present per decade within the at least one subrange of the frequency range by deleting at least one measurement frequency of the at least one subrange resulting in a second optimized frequency range is performed.
  • the method for adapting operation settings for a frequency sweep measurement of a polymer product method refers to special operation settings for the frequency sweep measurement that leads to significant reduction of measurement time while the method accuracy remains at an adequate level for the needs of plant control via fast frequency sweep.
  • the temperature is the same for both standard and special operation settings.
  • the test temperature is set to, for example, 190°C which is the same as for the MFI measurement.
  • Frequency range or equivalent shear rate
  • Low frequency measurements are the slowest (measurement point time is proportional to inverse frequency). Removing the low frequency measurements, leads to significant time reduction.
  • the frequency range is narrowed down from, for example, 628-0.01 rad/s to 250-0.1 rad/s.
  • Number of measurement points per decade This corresponds to the amount of measurement points measured per ‘decade’ (referring to the logarithmic scale) within the intended frequency range. This parameter has been changed from for example, 5 to 3 point/ decade.
  • settings lead to significant reduction of the measurement time.
  • the frequency sweep sample preparation and measurement time varies between 60 to 120 minutes, depending on the sample rheological characteristics, i.e. high viscosity polymers require higher measurement times.
  • the use of the above settings reduces the measurement time to a range of 10 to 15 minutes.
  • the method for adapting operation settings for a frequency sweep measurement of a polymer product refers offers an attractive method for use in the plant environment:
  • the Fast frequency sweep is able to provide the experimental results faster.
  • the sample preparation method is comparable to the currently employed melt index method.
  • the method for adapting operation settings for a frequency sweep measurement of a polymer product provides a more complete rheological insight on the complex shear viscosity curve compared to MFI that corresponds to a single point of the curve (at an unknown shear rate) and the acquired complex viscosity curve is a unique fingerprint for the characterized polymer, reflecting its microstructure in terms of MWD and comonomer content.
  • MFI may be misleading since different MWD may lead to the same MFI value.
  • the reduced shear rate range of the method still provides adequate feedback information for the scope of plant monitoring and control.
  • FIG. 2 shows a schematic diagram of an apparatus for adapting operation settings for a frequency sweep measurement of a polymer product according to an exemplary embodiment of the invention.
  • An apparatus 100 apparatus for adapting operation settings for a frequency sweep measurement of a polymer product is provided, the apparatus 100 comprises data memory 10 and a processor 20.
  • the data memory 10 is configured to provide at least one set of operation setting parameters comprising at least one frequency range for the frequency sweep measurement of the polymer product, the at least one frequency range comprising a plurality of specific measurement frequencies.
  • the processor 20 is configured to optimize the frequency range by deleting at least one measurement frequency of the plurality of specific measurement frequencies within a lower half of the frequency range resulting in a first optimized frequency range.
  • the processor 20 is configured to optimize the first optimized frequency range by determining a value of measurement frequencies present per decade of frequency within at least a subrange of the frequency range and reducing the determined value of measurement frequencies present per decade within the at least one subrange of the frequency range by deleting at least one measurement frequency of the at least one subrange resulting in a second optimized frequency range.
  • the processor 20 may be implemented as Digital Signal Processor, DSP, in a microcontroller or in any other side-processor or as hardware circuit within an application specific integrated circuit, ASIC, CPLD or FPGA.
  • DSP Digital Signal Processor
  • the processor 20 may be implemented as a Field Programmable Gate Arrays in terms of an integrated circuit that contains large numbers of identical logic cells.
  • the continuous need for advanced characterization methods for plant quality monitoring and control is well established.
  • a QC method able to exceed MFI capabilities but still able to be used in plant environment will enable better plant monitoring and control level to current polymer plants.
  • model predictive control is a powerful process tool, nevertheless, constant process feedback is needed in order to ensure the validity of the predictions.
  • melt index values are useful but not enough - MWD or complex viscosity over large shear rate range feedback is required. This way, the limited control feedback becomes a barrier for model predictive control steps.

Abstract

Procédé d'adaptation de réglages d'opération d'une mesure de balayage de fréquence d'un produit polymère, le procédé comprenant les étapes consistant : à fournir (S1) au moins un ensemble de paramètres de réglage d'opération comprenant au moins une plage de fréquences de la mesure de balayage de fréquence du produit polymère, l'au moins une plage de fréquences comprenant une pluralité de fréquences de mesure spécifiques ; à optimiser (S2) la plage de fréquences en supprimant au moins une fréquence de mesure de la pluralité de fréquences de mesure spécifiques dans une moitié inférieure de la plage de fréquences, ce qui permet d'obtenir une première plage de fréquences optimisée ; et à optimiser (S3) la première plage de fréquences optimisée par la détermination d'une valeur de fréquences de mesure présentes par décade de fréquence dans au moins une sous-plage de la plage de fréquences et la réduction de la valeur déterminée de fréquences de mesure présentes par décade à l'intérieur de l'au moins une sous-plage de la plage de fréquences par la suppression d'au moins une fréquence de mesure de l'au moins une sous-plage, ce qui permet d'obtenir une seconde plage de fréquences optimisée.
PCT/EP2023/053435 2022-02-14 2023-02-13 Procédé et appareil d'adaptation de réglages d'opération d'une mesure de balayage de fréquence d'un produit polymère WO2023152353A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP22156581.5 2022-02-14
EP22156581.5A EP4227663A1 (fr) 2022-02-14 2022-02-14 Procédé et appareil d'adaptation des paramètres de fonctionnement pour une mesure par balayage de fréquence d'un produit polymère

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WO2023152353A1 true WO2023152353A1 (fr) 2023-08-17

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EP (1) EP4227663A1 (fr)
TW (1) TW202346829A (fr)
WO (1) WO2023152353A1 (fr)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120312073A1 (en) * 2009-02-06 2012-12-13 Zevex, Inc. Air bubble detector
US20180045630A1 (en) * 2016-08-15 2018-02-15 New York University Method to estimate strain rate dependent elastic modulus of materials using dynamic mechanical analysis data
US20210277153A1 (en) * 2018-02-28 2021-09-09 Chevron Phillips Chemical Company Lp Advanced Quality Control Tools for Manufacturing Bimodal and Multimodal Polyethylene Resins

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120312073A1 (en) * 2009-02-06 2012-12-13 Zevex, Inc. Air bubble detector
US20180045630A1 (en) * 2016-08-15 2018-02-15 New York University Method to estimate strain rate dependent elastic modulus of materials using dynamic mechanical analysis data
US20210277153A1 (en) * 2018-02-28 2021-09-09 Chevron Phillips Chemical Company Lp Advanced Quality Control Tools for Manufacturing Bimodal and Multimodal Polyethylene Resins

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TW202346829A (zh) 2023-12-01

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